CN113830833A - Iron atom doping induction 1T-MoS2Graphene composite material and preparation method and application thereof - Google Patents
Iron atom doping induction 1T-MoS2Graphene composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses an iron atom doped induced 1T-MoS2A/graphene composite material, a preparation method and application thereof. The preparation method comprises the following steps: and dispersing and dissolving a molybdenum source and a sulfur source in a certain molar ratio in a certain volume of graphene dispersion liquid. The iron source solution is slowly added dropwise under the action of magnetic stirring, and a uniform mixed solution is formed under the action of magnetic stirring and ultrasound. Transferring the mixed solution to a polytetrafluoroethylene filmPressing the mixture in a reaction kettle, carrying out a high-temperature next hydrothermal reaction to obtain iron atom doped and induced 1T-MoS2A graphene composite material. The iron atom prepared by the invention is doped and induced to be 1T-MoS2The structure of the graphene composite material is ten to dozens of 1T-MoS2The nano sheets are stacked to form the three-dimensional spherical nanoflower, the three-dimensional spherical nanoflower is uniformly dispersed on the graphene substrate, and the composite material is rich in pores, large in surface area, high in 1T content, good in conductivity, stable in structure, excellent in electrolytic water hydrogen evolution activity and good in circulation stability.
Description
Technical Field
The invention belongs to the technical field of electrochemical catalytic materials, and particularly relates to iron atom doped induced 1T-MoS2A preparation method of a graphene composite material and application of the graphene composite material in hydrogen production through electrocatalytic decomposition of water.
Background
The serious environmental pollution and energy crisis worldwide have stimulated a great deal of attention to sustainable energy, including energy supply, energy storage, and clean energy technologies. Hydrogen has shown great advantages as a sustainable, clean energy source due to its zero emission and high energy density, which can overcome the problem of intermittent energy supply of other renewable energy sources (solar, wind, etc.). At present, methods for obtaining hydrogen energy include chemical treatment of fossil fuels, electrochemical decomposition of water to produce hydrogen, plant and microbial hydrogen production, waste decomposition, and the like. The electrochemical water decomposition is a clean and efficient hydrogen production method without discharging any pollution gas, and has attracted wide attention. The Hydrogen Evolution Reaction (HER) is an important technology for electrochemically decomposing water, and the hydrogen production process usually requires the assistance of a high-performance electrocatalyst. Platinum and palladium, as rare noble metals, have proven to be the most effective catalysts. However, high scarcity and high cost limit their large-scale application, and therefore the development of new efficient catalysts to replace traditional noble metal-based catalysts is the key to large-scale application of hydrogen energy.
In recent years, many non-noble metal catalysts, including metal oxides, carbon-based materials, two-dimensional materials such as graphene, two-dimensional Transition Metal Dihalides (TMDS), etc., have been explored for replacing platinum-based catalysts, particularly MoS2Since the gibbs free energy of hydrogen atom adsorption is close to that of platinum group metals, it is widely studied as a promising hydrogen evolution catalyst. Yet develop efficient, scalable MoS2Electrocatalysts, still face significant challenges. Studies have shown that according to MoS2Different arrangement of the sulfur atoms, MoS2There are two distinct crystalline phases: the conventional 2H phase (triangular prism structure) has semiconductor properties with a band gap of 1.3-1.9eV, while the 1T phase (octahedral structure) is a metallic conductor with 10% higher conductivity than the 2H phase7Multiple, thus 1T-MoS2Exhibits faster electron and charge injection/transfer characteristics and thus has better catalytic activity. Although metal 1T-MoS2It is very suitable for catalyzing the electrochemical hydrogen production of water due to its high conductivity, but it is difficult to produce stable 1T-MoS in large scale by ordinary chemical or physical methods2. In recent years, the improvement of MoS has been2A great deal of work is done on the aspect of catalytic performance, including reducing the size of the catalyst, constructing nanosheets rich in active centers, forming porous structures, doping heteroatoms, phase engineering, ensuring conductive substrates and the like. In general, the performance of a catalyst depends largely on the nature of the catalyst itself. Therefore, modulating the intrinsic electron/phase structure is an effective strategy for highly active catalysts. Currently, heteroatom doping has been extensively studied to modulate MoS2The performance has positive effects on the aspects of adjusting the electronic structure and exposing the active sites, thereby greatly improving the catalytic performance of the molybdenum disulfide. But in regulating MoS2The patent reports on the aspect of crystal structure are less, and the crystal structure is mainly applied to the aspects of super capacitors, energy storage and the like. For example, the invention patent 201910016729.0 discloses preparation and application of a tin-doped induced synthesized mixed-phase molybdenum disulfide-chlorella derived carbon composite material, wherein chlorella, a molybdenum source and a tin source which are prepared from certain raw materials in parts by mass are added into deionized water and rapidly stirred for 6-24 hours; drying the precipitate after centrifugation to obtain dark green blocky solid; weighing the obtained dark green block solid, adding sulfur powder, mixing at Ar 95%/H2Calcining in a 5% atmosphere tube furnace to obtain a black solid 1T-2H mixed phase molybdenum disulfide-chlorella derived carbon composite material, and using the black solid 1T-2H mixed phase molybdenum disulfide-chlorella derived carbon composite material as a negative electrode material of a sodium ion battery to show the characteristic of large-capacity sodium storage. The invention patent 201910627613.0 discloses a preparation method of carbon dot doping induced 1T phase molybdenum disulfide and application in energy storage materials, and the 1T phase molybdenum disulfide hybrid material prepared by reaction at 220 ℃ under high temperature and high pressure for 10 hours shows good electrochemical performance and catalytic wave-absorbing performance, and has wide potential of industrial application.
The method adopts heteroatom doping induction to synthesize the 1T-MoS2The material(s) of the material(s),however, the method has the disadvantages of various operation steps, difficult control and overhigh reaction temperature, and is applied to the aspects of super capacitors, energy storage and the like. Therefore, a safe, simple, low-cost and mild-reaction-condition method is designed for preparing the 1T-MoS with high stability and high activity2The method has great research value in expanding and applying to the hydrogen production by electrochemically catalyzing and decomposing water. The invention designs iron atom doped and induced 1T-MoS2The graphene composite material is successfully applied to the reaction of hydrogen production by electrochemically catalyzing and decomposing water, and no similar report exists at present, so that the graphene composite material has great research significance.
Disclosure of Invention
The invention aims to provide iron atom doped and induced 1T-MoS2A/graphene composite material, a preparation method and application thereof. The method takes non-noble metal iron as an inducer, selects cheap and easily-obtained raw materials, and prepares the iron atom doped induced 1T-MoS by a hydrothermal method at relatively low reaction temperature2The graphene electrocatalytic material has excellent hydrogen production performance by electrocatalytic decomposition of water and good circulation stability. The method has the advantages of simple process, strong operability, wide raw material source, low cost, large-scale production and accordance with environmental requirements.
The technical scheme adopted by the invention is as follows: iron atom doping induction 1T-MoS2The graphene composite material comprises the following specific steps:
(1) weighing a certain amount of graphene, dissolving the graphene in deionized water, and performing ultrasonic-assisted dispersion for 2 hours at room temperature.
(2) Weighing a certain amount of molybdenum source and sulfur source, adding into the graphene dispersion liquid obtained in the step (1), and stirring for 30min under magnetic force to fully dissolve the molybdenum source and the sulfur source.
(3) And (3) weighing a certain amount of iron source, dissolving the iron source in deionized water, slowly dropwise adding the iron source into the mixed solution obtained in the step (2) under the action of magnetic stirring, and performing ultrasonic treatment for 30min to fully dissolve and disperse the iron source.
(4) And (4) transferring the mixed solution in the step (3) to a polytetrafluoroethylene high-pressure reaction kettle, carrying out high-temperature reaction in a forced air drying box, taking out, and collecting a black product after the reaction kettle is cooled to room temperature.
(5) Centrifugally washing the black product with deionized water and absolute ethyl alcohol for 2-3 times in sequence, and drying in a vacuum drying oven to obtain iron atom doped induced 1T-MoS2A graphene composite material.
Preferably, in the step (1), the content of the graphene is 5mg to 60 mg. Further preferably, the graphene content is 25mg, and the volume of the deionized water is 20 mL.
Preferably, in the step (2), the molybdenum source is one or more of molybdenum trioxide, sodium molybdate dihydrate and ammonium molybdate tetrahydrate; the content of the molybdenum source is 0.1mmol-0.5 mmol. More preferably, the molybdenum source is ammonium molybdate tetrahydrate, and the content of the molybdenum source is 0.25 mmol.
Preferably, the sulfur source used in the step (2) is one or more of potassium thiocyanate, thiourea and thioacetamide; the molar ratio of the sulfur element in the added sulfur source to the molybdenum element in the molybdenum source is 2-5: 1. More preferably, the sulfur source used is thiourea and the molar ratio of elemental sulfur to elemental molybdenum is 3.5: 1.
Preferably, in the step (3), the used iron source is one or more of ferric trichloride hexahydrate, ferrous sulfate heptahydrate, ferroferric oxide and ferric nitrate, and the molar ratio of the iron element in the input iron source to the molybdenum element in the molybdenum source is 0.01-0.1: 1. Further preferably, the used iron source is ferric trichloride hexahydrate, the molar ratio of the iron element to the molybdenum element is 0.03: 1, and the volume of the deionized water is 10 mL.
Preferably, in step (4), the polytetrafluoroethylene autoclave filling rate is 60%. The heating temperature is 200 ℃, and the reaction time is 24 h.
Preferably, in the step (5), the vacuum drying temperature is 60 ℃, and the drying time is 8 h; the rotation speed of the centrifuge is 10000r/min, and the centrifugation time is 5 min.
The invention has the beneficial effects that:
the invention takes non-noble metal iron as an inducer, selects cheap and easily-obtained raw materials, and prepares the iron atom doped induced 1T-MoS by a hydrothermal method at relatively low reaction temperature2A graphene composite material. The invention has simple process, strong operability, low cost and iron sourceSuccessful induction of the daughter doping to generate 1T-MoS2And the graphene is well compounded with the graphene. The iron atom doped induced 1T-MoS-2/graphene composite material prepared by the invention has a structure of ten to dozens of 1T-phase MoS2The nano sheets are stacked to form the three-dimensional spherical nanoflower, the three-dimensional spherical nanoflower is uniformly dispersed on the graphene substrate, and the composite material is rich in pores, large in surface area, high in 1T content, good in conductivity, stable in structure, excellent in electrolytic water hydrogen evolution activity and good in circulation stability.
Drawings
FIG. 1 is an X-ray diffraction scan of samples prepared in examples 1 and 2 of the present invention.
FIG. 2 is a super-resolution field emission scan of a sample prepared in example 2 of the present invention.
FIG. 3 shows the Raman spectra of the samples prepared in examples 1 and 2 of the present invention.
Fig. 4 is a linear sweep voltammogram of the catalyst slurry prepared in the inventive verification example.
Detailed Description
The present invention will be described in detail with reference to specific examples, but the present invention is not limited to the embodiments in any way.
Example 1
0.3089g of ammonium molybdate tetrahydrate and 0.4662g of thiourea were weighed, dissolved in 30mL of deionized water under magnetic stirring, and then subjected to ultrasonic treatment for 30min to be sufficiently dissolved and dispersed. And transferring the mixed solution into a 50mL polytetrafluoroethylene high-pressure reaction kettle, putting the polytetrafluoroethylene high-pressure reaction kettle into an air-blowing drying oven, heating for 24h at 200 ℃, taking out, and collecting a black product after the reaction kettle is cooled to room temperature. And (3) centrifugally washing the black product with deionized water and absolute ethyl alcohol for 2-3 times in sequence, and drying the black product in a vacuum drying oven at 60 ℃ for 12 hours to obtain pure molybdenum disulfide.
Example 2
Weighing 25mg of graphene, dispersing in 20mL of deionized water, and performing ultrasonic-assisted dispersion for 2 hours at room temperature. 0.3089g of ammonium molybdate tetrahydrate and 0.4662g of thiourea were weighed and dissolved in the graphene dispersion solution under magnetic stirring for 30minIn the solution, 0.0142g of ferric chloride hexahydrate is weighed and dissolved in 10mL of deionized water, slowly and dropwise added into the graphene dispersion liquid under the action of magnetic stirring, and then the graphene dispersion liquid is subjected to ultrasonic treatment for 30min to fully dissolve and disperse the graphene dispersion liquid. And transferring the mixed solution into a 50mL polytetrafluoroethylene high-pressure reaction kettle, putting the polytetrafluoroethylene high-pressure reaction kettle into an air-blowing drying oven, heating for 24h at 200 ℃, taking out, and collecting a black product after the reaction kettle is cooled to room temperature. Centrifugally washing the black product with deionized water and absolute ethyl alcohol for 2-3 times in sequence, and drying the black product in a vacuum drying oven at 60 ℃ for 12 hours to obtain iron atom doped induced 1T-MoS2Graphene composite material (3% Fe-MoS)2/rGO-25mg)。
Verification example
The catalytic materials obtained in example 1 and example 2 were subjected to an electrocatalytic hydrogen evolution test: accurately weighing 5mg of catalytic material, dispersing in 980 mul of mixed solution of absolute ethyl alcohol and deionized water with the volume ratio of 1: 1, adding 20 mul of 0.5 percent naphthol solution, and performing ultrasonic dispersion for 2 hours to form uniformly dispersed suspension of 5 mg/L. Using Al for a glassy carbon electrode (GCE, diameter 3mm)2O3Polishing pretreatment is carried out on polishing powder (the particle sizes are 0.5 mu m and 0.05 mu m), ultrasonic washing is carried out on the polishing powder by deionized water and absolute ethyl alcohol in sequence, and a blower is used for blow-drying for later use. Transfer 5 mul of catalyst dispersion drop to cast on the pretreated glassy carbon electrode surface with a pipette and dry in an oven at 80 degrees celsius for 10 minutes. 0.5M H saturated with nitrogen using a three electrode system2SO4The test was performed in the electrolyte. The glassy carbon electrode modified by the catalyst, the platinum wire electrode and the saturated calomel electrode are respectively used as a working electrode, a counter electrode and a reference electrode. The linear sweep voltammetry curve test is performed in a voltage window of-0.4-0V in a concentration of 2mV s-1The sweeping speed of (2) is performed. As shown in FIG. 4, iron atom doping induces 1T-MoS compared to pure molybdenum disulfide2The graphene composite material shows more excellent electro-catalytic hydrogen evolution performance.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalents and modifications of the present invention based on the present invention are included in the protection scope defined by the present invention.
Claims (9)
1. Iron atom doping induction 1T-MoS2The graphene composite material is characterized in that non-noble metal iron is adopted to carry out doping induction on molybdenum disulfide.
2. Iron atom doping induction 1T-MoS2The graphene composite material is characterized by comprising the following steps:
(1) weighing a certain amount of graphene, dissolving the graphene in deionized water, and performing ultrasonic-assisted dispersion for 2 hours at room temperature.
(2) Weighing a certain amount of molybdenum source and sulfur source, adding into the graphene dispersion liquid obtained in the step (1), and stirring for 30min under magnetic force to fully dissolve the molybdenum source and the sulfur source.
(3) And (3) weighing a certain amount of iron source, dissolving the iron source in deionized water, slowly dropwise adding the iron source into the mixed solution obtained in the step (2) under the action of magnetic stirring, and performing ultrasonic treatment for 30min to fully dissolve and disperse the iron source.
(4) And (4) transferring the mixed solution in the step (3) to a polytetrafluoroethylene high-pressure reaction kettle, carrying out high-temperature reaction in a forced air drying box, taking out, and collecting a black product after the reaction kettle is cooled to room temperature.
(5) Centrifugally washing the black product with deionized water and absolute ethyl alcohol for 2-3 times in sequence, and drying in a vacuum drying oven to obtain iron atom doped induced 1T-MoS2A graphene composite material.
3. The preparation method according to claim 2, wherein the graphene content in the step (1) is 5mg to 60 mg.
4. The preparation method according to claim 2, wherein the molybdenum source in the step (2) is one or more of molybdenum trioxide, sodium molybdate dihydrate and ammonium molybdate tetrahydrate; the content of the molybdenum source is 0.1mmol-0.5 mmol.
5. The preparation method according to claim 2, wherein the sulfur source in the step (2) is one or more of potassium thiocyanate, thiourea and thioacetamide; the molar ratio of the sulfur element in the added sulfur source to the molybdenum element in the molybdenum source is 2-5: 1.
6. The preparation method according to claim 2, wherein the iron source used in the step (3) is one or more of ferric trichloride hexahydrate, ferrous sulfate heptahydrate, ferroferric oxide and ferric nitrate, and the molar ratio of the iron element in the added iron source to the molybdenum element in the molybdenum source is 0.01-0.1: 1.
7. The preparation method as claimed in claim 2, wherein the filling rate of the polytetrafluoroethylene high-pressure reaction kettle in the step (4) is 60-80%, the heating temperature is 170-210 ℃, and the heating time is 12-24 h.
8. The method according to claim 2, wherein the vacuum drying temperature in the step (5) is 50 to 80 ℃ and the drying time is 8 to 12 hours; the rotating speed of the centrifuge is 8000-10000r/min, and the centrifugation time is 3-8 min.
9. The iron atom doped induced 1T-MoS 2/graphene composite material of claim 2, wherein iron doping successfully induces synthesis of 1T-MoS2The composite material has a structure of ten to dozens of 1T-MoS2The nano sheets are stacked to form the three-dimensional spherical nano flower, are uniformly dispersed on the graphene substrate, have high 1T content, good activity and stable structure, and are successfully applied to the hydrogen evolution reaction of electrolyzed water.
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| CN116334683A (en) * | 2023-03-01 | 2023-06-27 | 浙江大学 | Fe doped MoS for bionic electrochemical nitrogen fixation 2 Preparation method of base nano material |
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| CN116334683A (en) * | 2023-03-01 | 2023-06-27 | 浙江大学 | Fe doped MoS for bionic electrochemical nitrogen fixation 2 Preparation method of base nano material |
| CN116334683B (en) * | 2023-03-01 | 2024-02-09 | 浙江大学 | Fe doped MoS for bionic electrochemical nitrogen fixation 2 Preparation method of base nano material |
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